CN112390291A - 一种钒酸盐助催化剂材料的制备方法 - Google Patents
一种钒酸盐助催化剂材料的制备方法 Download PDFInfo
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- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 13
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- 229940071125 manganese acetate Drugs 0.000 claims abstract description 6
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000003426 co-catalyst Substances 0.000 claims abstract description 3
- 239000011572 manganese Substances 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 16
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 10
- 229910052748 manganese Inorganic materials 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000001699 photocatalysis Effects 0.000 claims description 7
- 238000007146 photocatalysis Methods 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 5
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 5
- 229940043267 rhodamine b Drugs 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 5
- 229940082328 manganese acetate tetrahydrate Drugs 0.000 claims description 4
- CESXSDZNZGSWSP-UHFFFAOYSA-L manganese(2+);diacetate;tetrahydrate Chemical group O.O.O.O.[Mn+2].CC([O-])=O.CC([O-])=O CESXSDZNZGSWSP-UHFFFAOYSA-L 0.000 claims description 4
- 239000002957 persistent organic pollutant Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 claims description 2
- 238000006731 degradation reaction Methods 0.000 claims description 2
- 230000000593 degrading effect Effects 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229910003206 NH4VO3 Inorganic materials 0.000 claims 1
- 238000001556 precipitation Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 2
- 238000010923 batch production Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- 239000003054 catalyst Substances 0.000 description 11
- 230000000694 effects Effects 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000036961 partial effect Effects 0.000 description 3
- DYPHJEMAXTWPFB-UHFFFAOYSA-N [K].[Fe] Chemical compound [K].[Fe] DYPHJEMAXTWPFB-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000002574 poison Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- 238000001429 visible spectrum Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- ALTWGIIQPLQAAM-UHFFFAOYSA-N metavanadate Chemical compound [O-][V](=O)=O ALTWGIIQPLQAAM-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 229920000447 polyanionic polymer Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种钒酸盐助催化剂材料的制备方法,在本发明中将一定量的乙酸锰和偏钒酸铵溶于一定体积的蒸馏水中,加入适量的柠檬酸,搅拌,得到的混合溶液;将上述混合溶液转移至反应釜中,在烘箱中保温反应适当时间,待自然降温后,离心分离沉淀,沉淀放入烘箱中60℃烘干,得固体粉末,即为所述的一种钒酸盐助催化剂材料。本发明材料的制备过程简单,原料成本低,设备投资少,适合批量生产。
Description
技术领域
本发明属于材料化学领域,具体涉及到一种钒酸盐助催化剂材料的制备方法。
背景技术
助催化剂指本身不具活性或活性很小的物质,但能改变催化剂的部分性质,如电子结构、离子价态、酸碱性、表面结构、晶粒大小等,从而使催化剂的活性、选择性、抗毒性或稳定性得以改善。按助催化剂的功用,常分为:1)结构型助催化剂,用于增进活性组分的比表面积或提高活性构造的稳定性,如氨合成用的铁-氧化钾-氧化铝催化剂中的氧化铝;2)调变型助催化剂,可对活性组分的本性起修饰作用,因而改变其比活性,如前述铁-氧化钾-氧化铝催化剂中的氧化钾;3)毒化型助催化剂,能使某些引起副反应的活性中心中毒,从而提高目的反应的选择性,如在某些用于烃类转化反应的催化剂中,加入少量碱性物质以毒化催化剂中引起炭沉积副反应的中心。常用的助催化剂是掺入到金属氧化物催化剂中的金属离子,还原性或氧化性气体或液体,以及在反应过程中或在使用前加入到催化剂中的酸或碱。例如,合成氨的铁触媒里,加入少量铝和钾的氧化物,可使铁的催化活性增大10倍,延长寿命。
钒元素由于具有较多价态,能生成多种衍生物,形成各种骨架结构,如常见的V2O5和VO2,其中部分钒酸盐类化合物由于结合水的存在可以增强材料结构的稳定性,提高其催化氧化活性。部分钒酸盐作为助催化剂提高主催化剂的活性,可以减少贵金属主催化剂的用量,降低有机合成反应的成本。钒酸盐有正钒酸盐MVO4、焦钒酸盐MV2O7和偏钒酸盐MVO3等品种。这些盐都能从溶液中制取,将五氧化二钒溶于浓氢氧化钠溶液,可制得无色的钒酸钠溶液,其中钒以正钒酸根VO4 3-的形式存在。在水溶液中,随着溶液酸度的增加,钒酸根会以不同程度的缩合而形成组成不同的多阴离子。金属钒酸盐是一类优良的功能材料。除作为良好的基质材料广泛应用于荧光及激光材料领域,也可作为锂离子电池的阴极材料。最新的研究表明,某些钒酸盐在光催化领域存在着巨大的应用潜力,是一类新型的高活性光催化剂。利用TiO2光催化降解有机污染物是当前光催化领域的研究热点之一。但由于其带隙较宽(3.2 eV),需要紫外光来激发的缺点,很大程度上限制了TiO2的应用。为了克服这一缺点,一方面,人们通过各类掺杂技术改善TiO2对可见光谱的响应。少量的钒酸盐掺杂能改善TiO2对可见光谱的响应性能,其在光催化领域具有广泛的应用。
发明内容
本发明是针对现有技术,提供一种钒酸盐助催化剂的制备方法。
本发明为解决上述技术问题所采取的技术方案为:一种钒酸盐助催化剂的制备方法,其特征在于,所述制备方法采用以偏钒酸铵、乙酸锰为主要原料,加入适量的柠檬酸为表面活性剂调节水溶液pH值,在反应釜中进行水热合成,经过离心分离沉淀和烘干等处理,得到一种钒酸盐助催化剂,所述制备方法具体包括以下步骤:
1)称取一定量的偏钒酸铵(NH4VO3)和乙酸锰(Mn(CH3COO)2)溶于一定体积的蒸馏水中,然后加入适量的柠檬酸(C6H8O7),搅拌30min,得到混合物溶液;
2)将上述得到的混合物溶液转移至反应釜中,以10 ℃/min的升温速率在烘箱中将反应釜的温度升至160 ~ 180 ℃反应12 ~ 48 h;
3)反应结束后,自然冷却至室温,离心分离沉淀,沉淀放入烘箱中60℃烘干,得钒酸锰Mn3(VO4)2固体粉末,即为所述的一种钒酸盐助催化剂材料。
进一步的,本发明提供了一种钒酸盐助催化剂材料的用途,该材料作为TiO2光催化降解有机污染物罗丹明B的助催化剂,能够有效提高可见光降解效率,当TiO2中添加1%的所制得钒酸锰Mn3(VO4)2固体粉末材料,在可见光的照射下,10分钟内可降解罗丹明B染料达90%以上。
与现有技术相比,本发明的特点如下:
本发明通过水热反应一步法合成的钒酸锰Mn3(VO4)2性能优异,其作为助催化剂材料添加到TiO2光催化材料中,能够提高材料的光催化效率。
附图说明
图1为本发明制得的一种钒酸盐助催化剂材料的XRD图。
图2为本发明制得的一种钒酸盐助催化剂材料的SEM图。
具体实施方式
以下结合实施例对本发明作进一步详细描述。
实施例1
称取5.0 mmol(1.225g)乙酸锰·四水合物(Mn(CH3COO)2·4H2O)和10.0 mmol (1.19g)偏钒酸铵(NH4VO3)溶于25 mL的蒸馏水(H2O)中,加入0.5g的柠檬酸(C6H8O7),搅拌30 min,得到混合物溶液;将上述得到的混合物溶液转移至30 mL的反应釜中,以10℃/min的升温速率在烘箱中将反应釜的温度升至180 ℃保温12 h;反应结束后,自然冷却至室温,离心分离沉淀,沉淀放入烘箱中60℃烘干,得钒酸锰Mn3(VO4)2固体粉末,即为所述的一种钒酸盐助催化剂材料。将得到的钒酸锰固体粉末材料用X射线衍射仪测试其组成结构(图1);用扫描电镜SEM观测材料的形貌(图2)。
实施例2
称取7.5 mmol (1.838g)乙酸锰·四水合物(Mn(CH3COO)2·4H2O)和15 mmol (1.785g)偏钒酸铵(NH4VO3)溶于30 mL的蒸馏水(H2O)中,加入0.75g的柠檬酸(C6H8O7),搅拌30 min,得到混合物溶液;将上述得到的混合物溶液转移至50 mL的反应釜中,以10℃/min的升温速率在烘箱中将反应釜的温度升至160 ℃保温48 h;反应结束后,自然冷却至室温,离心分离沉淀,沉淀放入烘箱中60℃烘干,得钒酸锰固体粉末。将得到的钒酸锰固体粉末材料用X射线衍射仪测试其组成结构;用扫描电镜SEM观测材料的形貌。
实施例3
称取5.0 mmol(1.225g)乙酸锰·四水合物(Mn(CH3COO)2·4H2O)和10.0 mmol (1.19g)偏钒酸铵(NH4VO3)溶于25 mL的蒸馏水(H2O)中,加入0.5g的柠檬酸(C6H8O7),搅拌30 min,得到混合物溶液;将上述得到的混合物溶液转移至30 mL的反应釜中,以10℃/min的升温速率在烘箱中将反应釜的温度升至170 ℃保温24 h;反应结束后,自然冷却至室温,离心分离沉淀,沉淀放入烘箱中60℃烘干,得钒酸锰Mn(VO3)2固体粉末,即为所述的一种钒酸盐助催化剂材料。将得到的钒酸锰固体粉末材料用X射线衍射仪测试其组成结构;用扫描电镜SEM观测材料的形貌。
称取上述实施例所制得钒酸盐助催化剂材料0.1克,添加到10克TiO2粉末中,然后研磨混合均匀,形成混合物粉末,将所得的混合物粉末添加到浓度为1%的罗丹明B水溶液中,使用一千瓦的白炽灯模拟太阳光照射上述溶液,紫外光谱检测显示10分钟内降解罗丹明B染料可达90%以上。
Claims (3)
1.一种钒酸盐助催化剂材料的制备方法,其特征在于,所述制备方法具体包括以下步骤:
1)称取一定量的偏钒酸铵和乙酸锰溶于一定体积的蒸馏水中,然后加入适量的柠檬酸(C6H8O7),搅拌30min,得到混合物溶液;
2)将上述得到的混合物溶液转移至反应釜中,以10 ℃/min的升温速率在烘箱中将反应釜的温度升至160 ~ 180 ℃反应12 ~ 48 h;
3)反应结束后,自然冷却至室温,离心分离沉淀,沉淀放入烘箱中60℃烘干,得固体粉末,即为所述的一种钒酸盐助催化剂材料。
2.所述乙酸锰为乙酸锰·四水合物,其分子式为Mn(CH3COO)2·4H2O;
所述偏钒酸铵的化学式为NH4VO3;
所述钒酸盐助催化剂材料为钒酸锰,其化学式为Mn3(VO4)2。
3.一种如权利要求1所述的钒酸盐助催化剂材料的用途,其特征在于,该材料作为TiO2光催化降解有机污染物罗丹明B的助催化剂,能够有效提高可见光降解效率。
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